#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:21:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179106 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/68/4306865.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4306865
loop_
_publ_author_name
'Javier Vela'
'Jordi Cirera'
'Jeremy M. Smith'
'Rene J. Lachicotte'
'Christine J. Flaschenriem'
'Santiago Alvarez'
'Patrick L. Holland'
_publ_section_title
;
Quantitative Geometric Descriptions of the Belt Iron Atoms of the
Iron-Molybdenum Cofactor of Nitrogenase and Synthetic Iron(II) Model
Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              60
_journal_page_last               71
_journal_paper_doi               10.1021/ic0609148
_journal_volume                  46
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C39 H61 Fe N3'
_chemical_formula_sum            'C39 H61 Fe N3'
_chemical_formula_weight         627.76
_chemical_name_common            HOLJV54
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.8300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3029(7)
_cell_length_b                   16.3575(11)
_cell_length_c                   11.8844(8)
_cell_measurement_reflns_used    7988
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.267
_cell_measurement_theta_min      2.166
_cell_volume                     1936.2(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23593
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.029(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         9300
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0428P)²+0.0733P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                8672
_reflns_number_total             9300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0609148si20060525_034035_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4306865
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.828950(18) 0.651076(12) 0.752896(15) 0.02771(6) Uani 1 1 d . . .
N11 N 0.90976(12) 0.61903(7) 0.62040(10) 0.0271(2) Uani 1 1 d . . .
N15 N 1.02076(15) 0.68729(9) 0.86212(12) 0.0412(3) Uani 1 1 d . . .
N21 N 0.84039(13) 0.53542(8) 0.81591(11) 0.0309(3) Uani 1 1 d . . .
C11 C 1.05753(19) 0.53575(11) 0.53084(16) 0.0416(4) Uani 1 1 d . . .
H11A H 1.0083 0.5617 0.4580 0.062 Uiso 1 1 calc R . .
H11B H 1.0607 0.4765 0.5194 0.062 Uiso 1 1 calc R . .
H11C H 1.1492 0.5575 0.5539 0.062 Uiso 1 1 calc R . .
C12 C 0.88569(14) 0.67362(9) 0.52209(12) 0.0290(3) Uani 1 1 d . . .
C13 C 0.74828(18) 0.50935(10) 0.88205(15) 0.0380(4) Uani 1 1 d . . .
C14 C 0.66576(15) 0.72380(10) 0.74996(15) 0.0369(3) Uani 1 1 d . . .
H14A H 0.5964 0.7103 0.6779 0.044 Uiso 1 1 calc R . .
H14B H 0.6298 0.7065 0.8159 0.044 Uiso 1 1 calc R . .
C15 C 1.13149(19) 0.67916(11) 0.90892(15) 0.0416(4) Uani 1 1 d . . .
C21 C 0.98681(14) 0.55373(9) 0.62566(13) 0.0292(3) Uani 1 1 d . . .
C22 C 0.98218(16) 0.73155(10) 0.51021(14) 0.0348(3) Uani 1 1 d . . .
C23 C 0.62553(19) 0.47431(11) 0.82275(17) 0.0436(4) Uani 1 1 d . . .
C24 C 0.67742(16) 0.81741(11) 0.75555(14) 0.0376(4) Uani 1 1 d . . .
C25 C 1.27459(19) 0.66585(13) 0.96962(18) 0.0554(5) Uani 1 1 d . . .
C31 C 1.00547(15) 0.49514(9) 0.71497(13) 0.0319(3) Uani 1 1 d . . .
H31A H 1.0790 0.4590 0.7204 0.038 Uiso 1 1 calc R . .
C32 C 0.94923(18) 0.78574(11) 0.41652(16) 0.0432(4) Uani 1 1 d . . .
H32A H 1.0135 0.8251 0.4073 0.052 Uiso 1 1 calc R . .
C33 C 0.5361(2) 0.44879(14) 0.8865(2) 0.0585(5) Uani 1 1 d . . .
H33A H 0.4536 0.4236 0.8477 0.070 Uiso 1 1 calc R . .
C34 C 0.7359(2) 0.84846(13) 0.6583(2) 0.0584(5) Uani 1 1 d . . .
H34A H 0.8263 0.8260 0.6681 0.088 Uiso 1 1 calc R . .
H34B H 0.7405 0.9083 0.6611 0.088 Uiso 1 1 calc R . .
H34C H 0.6785 0.8311 0.5830 0.088 Uiso 1 1 calc R . .
C35 C 1.3499(2) 0.6476(3) 0.8767(2) 0.0852(8) Uani 1 1 d . . .
H35A H 1.3441 0.6951 0.8253 0.128 Uiso 1 1 calc R . .
H35B H 1.3094 0.6001 0.8308 0.128 Uiso 1 1 calc R . .
H35C H 1.4443 0.6361 0.9145 0.128 Uiso 1 1 calc R . .
C41 C 0.93114(15) 0.48235(9) 0.79711(13) 0.0314(3) Uani 1 1 d . . .
C42 C 0.82659(19) 0.78353(12) 0.33770(16) 0.0461(4) Uani 1 1 d . . .
H42A H 0.8068 0.8208 0.2742 0.055 Uiso 1 1 calc R . .
C43 C 0.5672(3) 0.46013(16) 1.0058(2) 0.0691(7) Uani 1 1 d . . .
H43A H 0.5059 0.4427 1.0485 0.083 Uiso 1 1 calc R . .
C44 C 0.7663(2) 0.84335(14) 0.87367(19) 0.0627(6) Uani 1 1 d . . .
H44A H 0.8582 0.8240 0.8813 0.094 Uiso 1 1 calc R . .
H44B H 0.7315 0.8196 0.9358 0.094 Uiso 1 1 calc R . .
H44C H 0.7664 0.9031 0.8797 0.094 Uiso 1 1 calc R . .
C45 C 1.2833(3) 0.5922(2) 1.0502(3) 0.0846(9) Uani 1 1 d . . .
H45A H 1.2325 0.6035 1.1079 0.127 Uiso 1 1 calc R . .
H45B H 1.3774 0.5817 1.0902 0.127 Uiso 1 1 calc R . .
H45C H 1.2454 0.5440 1.0043 0.127 Uiso 1 1 calc R . .
C51 C 0.9554(2) 0.40293(11) 0.86453(16) 0.0450(4) Uani 1 1 d . . .
H51A H 0.9808 0.4147 0.9482 0.068 Uiso 1 1 calc R . .
H51B H 1.0279 0.3726 0.8436 0.068 Uiso 1 1 calc R . .
H51C H 0.8732 0.3700 0.8455 0.068 Uiso 1 1 calc R . .
C52 C 0.73127(18) 0.72714(11) 0.35027(14) 0.0405(4) Uani 1 1 d . . .
H52A H 0.6462 0.7263 0.2953 0.049 Uiso 1 1 calc R . .
C53 C 0.6847(3) 0.49592(16) 1.06216(19) 0.0675(7) Uani 1 1 d . . .
H53A H 0.7034 0.5037 1.1440 0.081 Uiso 1 1 calc R . .
C54 C 0.5392(2) 0.85689(13) 0.7417(2) 0.0551(5) Uani 1 1 d . . .
H54A H 0.4813 0.8436 0.6648 0.083 Uiso 1 1 calc R . .
H54B H 0.5495 0.9163 0.7495 0.083 Uiso 1 1 calc R . .
H54C H 0.4986 0.8360 0.8021 0.083 Uiso 1 1 calc R . .
C55 C 1.3257(4) 0.7437(2) 1.0369(4) 0.144(2) Uani 1 1 d . . .
H55A H 1.2773 0.7526 1.0969 0.216 Uiso 1 1 calc R . .
H55B H 1.3107 0.7903 0.9833 0.216 Uiso 1 1 calc R . .
H55C H 1.4220 0.7383 1.0737 0.216 Uiso 1 1 calc R . .
C62 C 0.75763(15) 0.67160(9) 0.44196(12) 0.0315(3) Uani 1 1 d . . .
C63 C 0.7800(2) 0.52201(12) 1.00284(15) 0.0488(5) Uani 1 1 d . . .
C72 C 1.11965(16) 0.73775(11) 0.59686(16) 0.0406(4) Uani 1 1 d . . .
H72A H 1.1281 0.6916 0.6535 0.049 Uiso 1 1 calc R . .
C73 C 0.58736(18) 0.46139(12) 0.69236(17) 0.0455(4) Uani 1 1 d . . .
H73A H 0.6549 0.4908 0.6600 0.055 Uiso 1 1 calc R . .
C82 C 1.1337(2) 0.81791(12) 0.6652(2) 0.0541(5) Uani 1 1 d . . .
H82A H 1.0641 0.8208 0.7078 0.081 Uiso 1 1 calc R . .
H82B H 1.1237 0.8641 0.6112 0.081 Uiso 1 1 calc R . .
H82C H 1.2225 0.8202 0.7204 0.081 Uiso 1 1 calc R . .
C83 C 0.4493(2) 0.49701(18) 0.6344(2) 0.0699(6) Uani 1 1 d . . .
H83A H 0.4314 0.4911 0.5498 0.105 Uiso 1 1 calc R . .
H83B H 0.4475 0.5551 0.6544 0.105 Uiso 1 1 calc R . .
H83C H 0.3804 0.4677 0.6620 0.105 Uiso 1 1 calc R . .
C92 C 1.2345(2) 0.72995(16) 0.5355(2) 0.0605(5) Uani 1 1 d . . .
H92A H 1.2210 0.6805 0.4872 0.091 Uiso 1 1 calc R . .
H92B H 1.3207 0.7264 0.5940 0.091 Uiso 1 1 calc R . .
H92C H 1.2345 0.7780 0.4862 0.091 Uiso 1 1 calc R . .
C93 C 0.5922(3) 0.37159(15) 0.6612(2) 0.0726(7) Uani 1 1 d . . .
H93A H 0.6816 0.3496 0.6977 0.109 Uiso 1 1 calc R . .
H93B H 0.5738 0.3658 0.5765 0.109 Uiso 1 1 calc R . .
H93C H 0.5246 0.3414 0.6892 0.109 Uiso 1 1 calc R . .
C102 C 0.65275(16) 0.60955(11) 0.45512(14) 0.0366(3) Uani 1 1 d . . .
H10A H 0.6590 0.6050 0.5403 0.044 Uiso 1 1 calc R . .
C103 C 0.9090(2) 0.56273(14) 1.06764(16) 0.0587(5) Uani 1 1 d . . .
H10B H 0.9711 0.5629 1.0153 0.070 Uiso 1 1 calc R . .
C112 C 0.6828(2) 0.52487(13) 0.4139(2) 0.0611(6) Uani 1 1 d . . .
H11D H 0.7725 0.5075 0.4578 0.092 Uiso 1 1 calc R . .
H11E H 0.6794 0.5270 0.3308 0.092 Uiso 1 1 calc R . .
H11F H 0.6159 0.4858 0.4267 0.092 Uiso 1 1 calc R . .
C113 C 0.8841(3) 0.6517(2) 1.0958(2) 0.0939(8) Uani 1 1 d . . .
H11G H 0.8529 0.6826 1.0233 0.141 Uiso 1 1 calc R . .
H11H H 0.9678 0.6758 1.1424 0.141 Uiso 1 1 calc R . .
H11I H 0.8157 0.6537 1.1399 0.141 Uiso 1 1 calc R . .
C122 C 0.50877(19) 0.63581(17) 0.3959(2) 0.0667(7) Uani 1 1 d . . .
H12A H 0.4910 0.6894 0.4256 0.100 Uiso 1 1 calc R . .
H12B H 0.4457 0.5956 0.4125 0.100 Uiso 1 1 calc R . .
H12C H 0.4975 0.6392 0.3116 0.100 Uiso 1 1 calc R . .
C123 C 0.9793(4) 0.5160(2) 1.1794(2) 0.0954(10) Uani 1 1 d . . .
H12D H 0.9890 0.4583 1.1606 0.143 Uiso 1 1 calc R . .
H12E H 0.9253 0.5202 1.2361 0.143 Uiso 1 1 calc R . .
H12F H 1.0682 0.5397 1.2125 0.143 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N21 Fe1 N11 92.81(5) . . ?
N21 Fe1 C14 121.14(6) . . ?
N11 Fe1 C14 129.30(6) . . ?
N21 Fe1 N15 94.39(6) . . ?
N11 Fe1 N15 92.48(5) . . ?
C14 Fe1 N15 118.21(6) . . ?
C21 N11 C12 121.03(12) . . ?
C21 N11 Fe1 122.16(10) . . ?
C12 N11 Fe1 116.71(9) . . ?
C15 N15 Fe1 155.62(14) . . ?
C41 N21 C13 119.01(13) . . ?
C41 N21 Fe1 121.45(10) . . ?
C13 N21 Fe1 119.54(10) . . ?
C22 C12 C62 120.60(13) . . ?
C22 C12 N11 121.31(13) . . ?
C62 C12 N11 117.92(12) . . ?
C23 C13 C63 121.21(17) . . ?
C23 C13 N21 118.76(15) . . ?
C63 C13 N21 119.99(17) . . ?
C24 C14 Fe1 121.49(11) . . ?
N15 C15 C25 178.2(2) . . ?
N11 C21 C31 123.40(13) . . ?
N11 C21 C11 121.15(14) . . ?
C31 C21 C11 115.41(14) . . ?
C32 C22 C12 118.31(15) . . ?
C32 C22 C72 119.36(15) . . ?
C12 C22 C72 122.32(14) . . ?
C33 C23 C13 118.98(19) . . ?
C33 C23 C73 118.58(19) . . ?
C13 C23 C73 122.42(15) . . ?
C34 C24 C44 110.18(18) . . ?
C34 C24 C54 108.38(16) . . ?
C44 C24 C54 107.66(16) . . ?
C34 C24 C14 109.99(15) . . ?
C44 C24 C14 109.80(15) . . ?
C54 C24 C14 110.79(15) . . ?
C15 C25 C55 107.4(2) . . ?
C15 C25 C45 108.19(19) . . ?
C55 C25 C45 111.9(3) . . ?
C15 C25 C35 107.56(17) . . ?
C55 C25 C35 111.7(3) . . ?
C45 C25 C35 109.8(2) . . ?
C41 C31 C21 129.32(14) . . ?
C42 C32 C22 121.55(16) . . ?
C43 C33 C23 120.2(2) . . ?
N21 C41 C31 123.36(14) . . ?
N21 C41 C51 119.81(14) . . ?
C31 C41 C51 116.82(14) . . ?
C32 C42 C52 120.06(16) . . ?
C53 C43 C33 120.50(19) . . ?
C42 C52 C62 121.23(16) . . ?
C43 C53 C63 122.0(2) . . ?
C52 C62 C12 118.23(14) . . ?
C52 C62 C102 121.03(14) . . ?
C12 C62 C102 120.73(13) . . ?
C13 C63 C53 117.1(2) . . ?
C13 C63 C103 122.09(17) . . ?
C53 C63 C103 120.81(18) . . ?
C22 C72 C82 111.15(15) . . ?
C22 C72 C92 111.46(16) . . ?
C82 C72 C92 109.96(16) . . ?
C23 C73 C93 111.64(17) . . ?
C23 C73 C83 112.09(17) . . ?
C93 C73 C83 110.1(2) . . ?
C62 C102 C112 111.39(14) . . ?
C62 C102 C122 113.32(15) . . ?
C112 C102 C122 111.04(18) . . ?
C63 C103 C113 110.9(2) . . ?
C63 C103 C123 112.2(2) . . ?
C113 C103 C123 110.5(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N21 2.0269(13) . ?
Fe1 N11 2.0294(12) . ?
Fe1 C14 2.0526(16) . ?
Fe1 N15 2.1513(15) . ?
N11 C21 1.3227(19) . ?
N11 C12 1.4407(19) . ?
N15 C15 1.142(2) . ?
N21 C41 1.3360(19) . ?
N21 C13 1.443(2) . ?
C11 C21 1.519(2) . ?
C12 C22 1.406(2) . ?
C12 C62 1.416(2) . ?
C13 C23 1.403(3) . ?
C13 C63 1.404(2) . ?
C14 C24 1.536(2) . ?
C15 C25 1.482(3) . ?
C21 C31 1.406(2) . ?
C22 C32 1.395(2) . ?
C22 C72 1.526(2) . ?
C23 C33 1.398(2) . ?
C23 C73 1.513(3) . ?
C24 C34 1.521(3) . ?
C24 C44 1.527(2) . ?
C24 C54 1.533(2) . ?
C25 C55 1.524(4) . ?
C25 C45 1.528(4) . ?
C25 C35 1.533(3) . ?
C31 C41 1.402(2) . ?
C32 C42 1.367(3) . ?
C33 C43 1.384(4) . ?
C41 C51 1.513(2) . ?
C42 C52 1.383(3) . ?
C43 C53 1.357(4) . ?
C52 C62 1.391(2) . ?
C53 C63 1.414(3) . ?
C62 C102 1.519(2) . ?
C63 C103 1.509(3) . ?
C72 C82 1.529(3) . ?
C72 C92 1.546(3) . ?
C73 C93 1.519(3) . ?
C73 C83 1.528(3) . ?
C102 C112 1.527(3) . ?
C102 C122 1.532(3) . ?
C103 C113 1.530(4) . ?
C103 C123 1.543(3) . ?
